Process of and apparatus for distilling crude pine-resins.



APmlcArlon msn MN. i2. ma. y 1,291,800.; Patented Jan. 21,1919.

vinvITED STATES PATENT OFFICE.

BOBSON DUN'WODY;A OF NEW ORLEANS, LOUISAiNA.

PRCESS 0F AND APRBTUS FOR-D1`STILLING GRUDE 'PINE-RESINS. l

Secilcation of Letters Patent.

Application mea January 12, 191s. serial No. 211,552.

To all wkom t may concern `Be it known that I, RosoN Dnnwon,

y a citizen of the United States, residing at Resins arid lido hereliyeclare thei'follow- )i i Seite. of Louisiana,

New Orleans,.in the 1parish of Orleans and of andApparatus for Di'stilling Crude Pine ing to beaa full, clear, ,and exact description 4 ave invented, certain new and useful Improvanents 1n Processesof the invention, such 'as will enable others skilled in the art'to vv'hichv it appertains' to make and use the' same. 4

This inventionrelates to a method of and V an apparatus for' distilling crude pi'nere'sins and" has for its object to improve the methods and a paratus heretofore proposed.

Wi these and'v other objects in'view the invention consists in the novel steps and combinations of steps constituting the process' and in the' novel parts and' combinations of parts constituting the apparatus all as l will be more fully hereinafter disclosed and particularly pointed out in the claims.

y Referrin to' the accompanying drawing vlin'edbottom 2O of the filter 7 to the pipe 21 leading into the drippings tank 22, and 23 reperesents any suitable valve for con trolling the passage of material through said connection 19. 25 represents a connection from the upper portion of the filter 7, to

resin or gum is given a vigorous mechanical y stirring through the means 4 and its lumps in' which t e gure is a diagrammatic view i partly in, section' of an apparatus ni'ade'in accordance with this invention, 1 indicates in? suitable' preheater for the resins proedi the openings 2,. throu li which said'l resins may be"int1oduced as yellow ing the'same to fiow from the barrels conl aining'the same, 3 any suitable preheatiso ing means such us a steaxncoil for example, el: any suitable'stirring apparatus, and 5 a valve controlling the connection 6 extending between the preheuter 1 and the filtering apparatus 7. The snid filteringl or straining apparatus 7 preferably comprises a relntively coarse screen or strainer 8 having sny one inch meshes made of Wire cloth, a scc ond screen' or' filter`- 9 having finer' meshes .say one fourth inch, also made ofwire cloth, and a third screen or strainer 10 likewise made of .wire .cloth and having meshes made say one t'ent'hv of an inch in size, although any form of filter' or 'centrifugal o1'- other method of separating the' dross from the gum may be used.

11 indicates a valve controllingv aconnection 12 between the filter 7 and passage or connection I3, ledin to the still or kettle 14. The said still or yKettle is provided with any suitable cover 15 and any suitable outlet 16 controlled by a valve 17. 1S represents any suitable receptacle for the', resin. '19 represents a diinectioil ledtigfrom the inmore orl less broken up. The molten 'gum thus heated is next Iled through the connection 6 .when it flows down along and over the relatively coarse screen 8,through the meshes of which a portion of said gum passe'sand' is caught on the .fine-r meshes of the screen That portion of the gum which docs not pass through the' meshes of the screen 8 passes down over the end of said screen through the space 40 and thus reaches the screen 9. Another portion of lthe gum will pass p Patented J an. 21, 1919.

through the meshes of the next coarserv screen 9 and still. another portion thereof will passthrough the space 41 at the end of said screen 9 whereupon rvthe molten gnni will reachv the screen 10 and pass through its meshes, fillingl up the space 4B above the inclined bottom 20. Stated in otig'lr language, the gum as it enters thefilter 7 is in the form of a viscous, sticky, liquid .but thin enough to How rather freely; so ythat 'it quickly passes through the screens to the space 43, and on into the kettle or still 14. Accordingly, although the ten'iperature is somewhat higher than in the `preheater 1, yet, these first runnings of the gum have not been subjected to this higher temperature for a time sufiiciently long to bring out the stains to any eat extent. It results that substantially a l the discoloring material remains behind with the foreign, matter which adheres 'to the screens, and a very 'high grade of gum isseparatedout and passed ntothe still414, f0r the valve 23' being closed the grim filliiig'the space. 43" cannot escape through the connection 19, and therefore, the cleaner-uncolored, unstained and purer portions of the gum will lill the connection 12 vand the valve 11 being opened it will'pass through the connection 13 into the still 14. In the meantime, the woody particles, sand, dir-t, and other refractory lumps of gum, etc., deposited on the various screens 8, 9, and 10, and the gum associated `therewith is recovered in a manner to be disclosed below.

When a suiicient amountof substantially pure unstained, uncolored gum has been thus l deposited in the sill 14, the valve 5 1s closed and the valve 23 is opened. The stillbeing redup the distillate consists ofA sp1 tits of turpentine and an acid Water known 1n the trade as low Wine, there being other oils and xnpuritles present in nnnor quantities, The ,n

vapors of this distillatev Will now pass through the filter box 7 and through the screens 10, 9 and 8 containing the above nientioned impurities and said vapors will pass on throughthe connection 25 into the condenser 26. The vapors of said distillato being condensed in the condenscrll they are` led through the connection 27 into the separater 28 ,Where the low wine'is permitted to go to waste through the connection i9 ,and the turpentine is led through connection 29 lo the receiver 30. In the n'ieantin'ie, the :5t

I. tlv d the io and 10, factory linups that may rest thereon. The said dissolved ,gum vnow trickles down and reaches the space 425 and is led troni time to time into the filter drippings tank 22 by opening the valve 23 andl thus only the unstained substantially pure, material Ais alolve all the resins or gum from les resting upon the screens 8 lowed to enter the still l-i. ln fact the xnaterials i 43 and pi sing; thc valve 23 will be found to contain substantially' all the roloring matter that has been extracted trointhe chips and other" impurities carried by the gum and thus he material that passes into the still 14 will be substantially Free from all coloring matter. :which would not he [he caseiii no sloping bottoni 2O were provided. That ist() say, although this said sloping,r bottom does,

no! collect the, stained portions of the 1uni during the first rnnnings of' unstained yet. il docscollcf' ihr land` dirt and other heavy and small parliclesot' foreign matterj which pas:` the fillers during the earlystagesn 0f the process and thus prevents this inalc-A rial from contaminating' the high grade. ,quin inthe still lll.

completed in the still lai the valve i7` is opened and the, residue, in thekettle. `whi\h is commercial rosin, is led into thelter or rosin receptacle 18. The rosin isconifenientlyy drawn from said'reeeptacle 18, by any,r`

'l hot vapors of lowl wine and turpentine f and they further dissolve anyv re- "llecled at the bottoni of thespaco,

gum,

, y Y Ik l". When the distillation process has been suitable connection not shown into barrels read for shipping. rl`he dry sknonnngs When lsulii'ci'e'nt gum has been collected in the drippings tank to make a charge it may be independently distilled.

Itwill now be clear that by -lollowing the process outlined instead ot' t'ollowin, y the processes heretofore employed. I am able to segregate with celerityand certainly, all the foreign matter that is .generally collected with the crude vn'xaterial and which causes 1 considerable loss in the quality of the product; That is to say,und`er the method of distillation prior to this invention. the crude entail a considerable loss which vis a-'oidcd i by following the above process.,

In addition to this, therelis a considerable loss of turpentine vapors escaping from the still during the skimming process, while in the processdiselosed above, the still and theI other apparatus being closed, no such loss occurs. v Not only inthe prior processes are theabove losses of `material experienced, but the chips, bark, straw, etc., with which the-crude gum is Agenerally associated has the eifeotduring the distillation process ot staining .thea'osin and thus causing it to he.

sold inthe market. at a V much lower grade than it lwould he sold at. il said stains did not exist. v y

.By my process, on the yother hand, it will be observed that. owing to the separating out of the, colored or stained portion of the gunrfrom. the yunstaineol portioml am enabled-to, produce a much higher ,grade of ,rosin vthan would otherwise ybe possible. Not .only does the staining of` the. rosin thus `left in the filter hok T on the screens S. 9 and l 10 may now be removed and destroyed.

lower its grade, but these foreign materials ...sometimesaccumulate-in the kettle in such heavy layers esto, make the heatingof. the

, mass ,quitediiiicult to control and therefore v`a scorchingoffthe, charge is often k,expel-ii `encedl and thus, therosin is `still further floweredyin grade .,while,a` still 'further loss ,of time andmateriah isrntailed., lt will @thus he seen that my process a voids these .last mentioned.obiections also, Again. eren illitlra mostrar-cfu] skinnninp'ofthe male ,rrah now,v practised, 1t is rnnpossible to remove all thechips, bark, 'strawetc., and it 130 fi @el ,ieee

is further impossible to remove `any suhstanl tiel portion/of the sand, dirt, 'line particles of charcoal,` etc. By my process, as above stated, :these objections cre-entirely avoided. lt `is true that-*efforts have been heretofore made to filter the crude gum before putting it into ftlie still, but so :for as 'I am awa-re, they have all been failures commercially in that When'thoy yreinovedthe chips, dirt, etc., mentioned above, they also removed the reractory herd lumps or so called resin acid crystals lor scrape along with said chips, etc., end thus entailed a heavy loss which is not exwericnced in my process.

t has been further proposed Ato collect the skimmings consisting of gum or rosin saturated chipsyberk, dirt, resin, acid crystal scrape7 etc., saturated with 'gum and crystals, or \refractory lumps.

to seperately 'tr/eatftiie saine to recover the valuniole products present, but all such-procceses, in soltar yasl am aware hsvebeen coinmercial failures in that Wliere'this hasbeen tried at "the distillery, steaming or other process was used that was nnsuccessul. 'Gr when an effort was lmade totieatlthese at some central planteqnipped with more eilicient appamtua ysuch as solvent preeess,'tlie cost of transportation and` collection 'has been so 'greet es moet ina'ill p1 o'ts in the procedure and therefore 'the practical man lies lonnd it best to simiy let 'suoli skiinniings Ago to Waste. v)By my ,process on the other hand, suhstantia'prots 'are easily bteined by 'treating-these impurities at 4the distillery. An important feature rif-*this invention resides in lthe "factthat these said gum lumps, scrape skimniiigs, etc., are treated with the hot va ors of distillation. These said vapors readi y dissolves out the gum present on the skimmings without en toiling any loss at all when my process is involved While with the'other processes here: tofore proposed not only has the dissolving action been imperfect 'but it has also en- Y tailed a considerable loss of material.

Il, Willtherefore be seen that by following the shove mentioned process I subject the crude gum as it comes from the trees and which is associated with more or less quantities of chips, bark, charcoal, sand, dirt, scrape or refractory lumps of gum, etc., to n preheater and to a mechanical stirring or agitation which serves to uniformly mix the material and to break np and to dissolve up` as much es possible the said gum Second I separate ont these impurities and refractory portions of the gum.

flhird I next subject the strained and i1n- .stained gum to n distilling action and utilize the vapors of the distillate to dissolve the @gum and the refractory lumps of gum and resin acid crystals out of the skimmings whereupon the seid vapors also paw on through the condenser and into the seperator 28 whore 'the 'flow 'wine and water portions ofthe distillate are separated from the t turpentine portions midfthe turpentineis Afinally Arecovered in the Flink in the meantime it willbe observedthat the gum recovered 'from fthe--skinnnin'gsf and `which is diseolored from stains and'fixnputies is collected for :it convenience. y

'The heating/notion intheprelieatcr '1 is pentine and I prefer toiinterpse a Jsuction fan 55 or some otheri'ncansbetween said preheater 1 and thecondegnseQ in orderto i deliver such vapors .tinto said condenser, but

while at -the seme/time 'b- 'recoveringgthe separate' treatment or distillation rosin and the'turpenlniet1 rom Vthe tiros/sill avoid any loss of inaterlil."Y y@he whole-japparatns constituting a *closed Lthere -is' a minimumloss ofamateriitl. j ji It is obviousithat those skilled inthefrt may vary the details of the process ns Well as the details of. the construction and arrangement of parts without departin "from the spirit ofA he invention and'thcr 'ore.,"I

donot Wishitobe'limited to the above disclosure except as may heyreqn'ired byl'the claims.

Wiehl claim is 1. The steps in n process ofvproducing'turpentine and rosin from crude gum materials `which'consists in preheating said materials;

ngitnting said preheated materials to produce a more uniform mixture and to par-I tially break up any refractory lum s that might exist; suitably straining or ltering seid preheated and agitated materials; separating the colored or stained material from the portions not colored; subjecting the uncolored portions of said strained materiel to a distilling action; and causing the vapors of distillation to pass through the residue to dissolve ont any gum that niay be present therein; substantially as described.

2. The process of producinjlg tnrpentine and rosin from crude gums which consistsl in melting and stirring said gum; then passling; said melted gum through a strainer or filter; automatically Separating the unstnincd from the stained portions of said gum; distilling the gum to 4separate out the rosin present; passing the vapors of the distillate through the material left on the said strainer to dissolve out any gum present; condensing said vapors; and separating out the turpentine present, substantially as described.

vstrainers of different mesh; separating the '3. The process of producing turpen'tine and rosin from crude gum which consists in passing said gum through a plurality of strainers of dilerent mesh; ,separating the unstained from the stained portions of the .gum; distilling the unstained portion of said stained from the unstained portions of the gum; di'stilling one of said portions to separate out its rosin; passingv the vapors of the distillate through said strainers to dissolve any gum present; adding the dissolved gum thus obtained to the stained portions of the gum; and recovering the turpentine from boththe stained and unstained portions of said gum, substantially 'as described.

v5. In an apparatus for distilling crude gum the combination of a preheater; a filter connected to said preheater and having an 'inclined bottom; a still having its vapor outlet connected to said ilter nearAthe highest point of 'said bottom; a condenser connected to said filter near its top; a separator connected to said condenser; and a turpentine receiver connected to `'said separator the Whole so arranged that the stained'portions of the gum'may be separated from the un-` stained portions thereof, and the vapors from said still may pass through rand disf provided with a screen and van inclined bottom below said screen connected tosaid preheater; a still connected to said filter above said inclined bottom and below said screen; and a condenser Aconnected to said filter above said screen, whereby the vapors from said still may pass through and dissolve the gum left on said screen and whereby solids and other impurities are collected on said inclined bottom, substantially :as-described.

7. In an apparatus for distilling crude gumthe combination of a preheater; a lter connected to said prelieater and having an inclined bottom; a drippings tank connected to said inclined bottom at its lowest point; a still connected to said filter near the highest point of said bottom; a. turpentine receptacle; a condenser; a separator; a connectionbetween thebottom of said condenser and said separator; a connection between said turpentine .receptacle and said separator;

an'd a connection between the top portion ot said condenser and said ilter, whereby the 1 vapors from said still may pass through and dissolve the gum left in said lter, substan 

